CN106957179B - SiBN fiber reinforced SiO2-BN-Al2O3Preparation method of wave-transparent composite material - Google Patents
SiBN fiber reinforced SiO2-BN-Al2O3Preparation method of wave-transparent composite material Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 52
- 239000000835 fiber Substances 0.000 title claims abstract description 49
- 229910003697 SiBN Inorganic materials 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title abstract description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 45
- 238000005470 impregnation Methods 0.000 claims abstract description 37
- 238000001035 drying Methods 0.000 claims abstract description 33
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 26
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 26
- 238000005245 sintering Methods 0.000 claims abstract description 24
- 239000011268 mixed slurry Substances 0.000 claims abstract description 21
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 17
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims description 29
- 238000010438 heat treatment Methods 0.000 claims description 18
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 10
- 229910052582 BN Inorganic materials 0.000 claims description 5
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 5
- 239000000843 powder Substances 0.000 abstract description 19
- 238000002679 ablation Methods 0.000 abstract description 4
- 238000009991 scouring Methods 0.000 abstract description 4
- 239000012467 final product Substances 0.000 abstract 1
- 239000010453 quartz Substances 0.000 description 15
- 239000002002 slurry Substances 0.000 description 9
- 229910052681 coesite Inorganic materials 0.000 description 5
- 229910052906 cristobalite Inorganic materials 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 229910052682 stishovite Inorganic materials 0.000 description 5
- 229910052905 tridymite Inorganic materials 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 238000000498 ball milling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000001272 pressureless sintering Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
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- C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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- C04B2235/3852—Nitrides, e.g. oxynitrides, carbonitrides, oxycarbonitrides, lithium nitride, magnesium nitride
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Abstract
The invention relates to SiBN fiber reinforced SiO2‑BN‑Al2O3The preparation method of the wave-transparent composite material comprises the steps of adding nanometer BN powder and nanometer Al into silica sol2O3Uniformly stirring the powder to obtain mixed slurry; placing the SiBN fiber prefabricated member in mixed slurry for vacuum impregnation, wherein the impregnation pressure is 20-60 KPa, and then drying and sintering to obtain a composite material after sintering; placing the sintered composite material in mixed slurry for pressure impregnation, wherein the impregnation pressure is 2-8 MPa, and then drying and sintering; repeating for 4-6 times to obtain the final product. The invention has the advantages of simple process, easy operation, low cost, high density of the composite material, excellent dielectric property, high ablation resistance and strong scouring resistance.
Description
Technical Field
The invention belongs to the field of preparation of wave-transparent composite materials, and particularly relates to SiBN fiber reinforced SiO2-BN-Al2O3A method for preparing a wave-transparent composite material.
Background
The wave-transmitting material is a multifunctional medium material used for an aircraft antenna window/cover to protect the aircraft antenna window/cover to complete tasks such as communication, telemetering, guidance and the like in a severe service environment. The quartz fiber reinforced quartz wave-transparent composite material has the advantages of strong ablation resistance, low thermal conductivity, good dielectric property and the like, and is one of the commonly used high-temperature wave-transparent composite materials. However, the quartz fiber reinforced quartz wave-transmitting composite material also has the defects of low density, high porosity, easy moisture absorption and the like, particularly, the quartz fiber begins to generate a crystallization phenomenon at about 900 ℃, the fiber strength is rapidly reduced at high temperature, the strengthening and toughening effects of the quartz fiber are weakened, and the composite material strength is lower at high temperature. In order to prepare wave-transparent composite materials with more excellent high-temperature mechanical properties, various improvement measures are applied, wherein matrix doping complex phase modification treatment is mainly adopted.
Chinese patent CN102167609A (published as 2011, 8, 31) discloses a quartz/quartz-boron nitride high-temperature wave-transmitting material and a preparation method thereof, wherein the method uses quartz fiber fabric and SiO2The sol is used as a raw material, a sol-gel process is adopted to prepare a quartz/quartz ceramic blank, and then the quartz/quartz ceramic blank, boric acid, urea and ethanol are used as raw materials to be subjected to vacuum impregnation and pressureless sintering to obtain the quartz/quartz-boron nitride high-temperature wave-transmitting material.
Chinese patent CN103964860A (published as 2014, 8, 6) discloses a boron nitride-based wave-transparent composite material prepared by hot pressing with nanometer silica sol as sintering aid and a preparation method thereof, wherein amorphous nanometer SiO is used in the method2Mixing with hexagonal boron nitride powder, and adding ethanol and ZrO2And performing ball milling on the ceramic balls serving as a ball milling medium to prepare slurry, grinding and sieving to obtain a mixed material, and performing a sintering process to obtain the boron nitride-based wave-transparent composite material. The method has the advantages of simple preparation process and controllable process, and has the defect that the toughness of the obtained composite material is lower because wave-transmitting fibers are not adopted as a reinforcing phase.
Chinese patent CN103664215A (published as 2014, 3, 26) discloses a method for preparing quartz fiber toughened multiphase ceramic wave-transparent composite material, which comprises soaking quartz fiber preform in a solution containing nanometer SiO2、Si3N4And Al2O3And drying the sol of the powder, and sintering to obtain the multiphase wave-transparent composite material. The method has the advantages of being processedThe preparation method has the advantages of relatively simple process, low cost, good toughness and excellent dielectric property, and has the defect of low high-temperature mechanical property and anti-scouring property of the composite material.
Disclosure of Invention
The invention aims to solve the technical problem of providing SiBN fiber reinforced SiO2-BN-Al2O3The invention relates to a preparation method of a wave-transparent composite material, which is SiBN fiber reinforced SiO with high-temperature mechanical property, ablation resistance and scouring resistance and excellent wave-transparent property2-BN-Al2O3A wave-transparent composite material.
The invention relates to SiBN fiber reinforced SiO2-BN-Al2O3The preparation method of the wave-transparent composite material comprises the following steps:
(1) adding nanometer BN and nanometer Al into silica sol2O3Uniformly stirring to obtain mixed slurry;
(2) placing the SiBN fiber prefabricated member in mixed slurry for vacuum impregnation, wherein the impregnation pressure is 20-60 KPa, and then drying and sintering to obtain a composite material after sintering;
(3) placing the sintered composite material in mixed slurry for pressure impregnation, wherein the impregnation pressure is 2-8 MPa, and then drying and sintering;
(4) repeating the steps (2) and (3) for 4-6 times to obtain SiBN fiber reinforced SiO2-BN-Al2O3A wave-transparent composite material.
SiO in the silica sol in the step (1)2The mass percentage of (A) is 20-30%.
SiO in the silica sol in the step (1)2The average particle diameter of the particles is 10-15 nm, the average particle diameter of the nano boron nitride BN is 100-200 nm, and the nano Al2O3The average particle diameter of the particles is 30 to 60 nm.
The silica sol, the nanometer BN and the nanometer Al in the step (1)2O3The mass ratio of (8-12) to (1-4) to 1.
The SiBN fiber prefabricated member in the step (2) is in a 2.5-dimensional woven or 3-dimensional braided structure.
The volume fraction of the fiber in the SiBN fiber prefabricated part in the step (2) is 35-50%.
The drying in the steps (2) and (3) is as follows: raising the temperature from room temperature to 100-120 ℃, wherein the heating rate is 0.5-1 ℃ per minute, and then preserving the heat for 20-40 minutes at 120-140 ℃.
The sintering in the steps (2) and (3) is as follows: sintering at 800-1000 deg.c for 1-2 hr.
Advantageous effects
(1) The preparation method is simple, easy to operate and low in cost;
(2) the composite material has high density, excellent dielectric property, high ablation resistance and high scouring resistance.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
(1) Preparing SiBN fiber into a 3-dimensional woven prefabricated part structure, wherein the fiber volume fraction of the prefabricated part is 35%;
(2) in SiO2Adding nanometer BN powder and nanometer Al into silica sol with the mass percent of 20%2O3Powder of, among them, silica sol, nano BN powder and nano Al2O3The mass ratio of the powder is 10:2:1, and after uniform stirring, mixed slurry is obtained, wherein SiO is contained in silica sol2The average particle diameter of the particles is 10-15 nm, the average particle diameter of the added nano BN is 100-200 nm, and nano Al2O3The average particle diameter of the particles is 30 to 60 nm.
(3) Placing the SiBN fiber prefabricated member in the mixed slurry for vacuum impregnation, wherein the impregnation pressure is 20 KPa;
(4) and (3) placing the SiBN fiber prefabricated member after the slurry impregnation into a drying box for drying treatment process. The drying treatment process comprises the steps of heating from room temperature to 100 ℃, heating at the rate of 0.5 ℃ per minute, and then preserving heat at 120 ℃ for 20 minutes;
(5) placing the dried composite material at 800 ℃ for sintering treatment for 1 hour;
(6) placing the sintered composite material in the mixed slurry for pressure impregnation, wherein the impregnation pressure is 2 MPa;
(7) and (3) placing the composite material after the slurry impregnation in a drying box for drying treatment. The drying treatment process comprises the steps of heating from room temperature to 100 ℃, heating at the rate of 0.5 ℃ per minute, and then preserving heat at 120 ℃ for 20 minutes;
(8) placing the dried composite material at 800 ℃ for sintering treatment for 1 hour;
(9) repeating the steps (3) to (8) for 4 times to obtain SiBN fiber reinforced SiO2-BN-Al2O3A fundamental wave-transparent composite material.
Example 2
(1) Preparing SiBN fiber into a 3-dimensional woven prefabricated part structure, wherein the fiber volume fraction of the prefabricated part is 40%;
(2) in SiO2Adding nanometer BN powder and nanometer Al into 25 mass percent of silica sol2O3Powder of, among them, silica sol, nano BN powder and nano Al2O3The mass ratio of the powder is 8:3:1, and after uniform stirring, mixed slurry is obtained, wherein SiO is contained in silica sol2The average particle diameter of the particles is 10-15 nm, the average particle diameter of the added nano BN is 100-200 nm, and nano Al2O3The average particle diameter of the particles is 30 to 60 nm.
(3) Placing the SiBN fiber prefabricated member in the mixed slurry for vacuum impregnation, wherein the impregnation pressure is 35 KPa;
(4) and (3) placing the SiBN fiber prefabricated member after the slurry impregnation into a drying box for drying treatment process. The drying treatment process comprises the steps of heating from room temperature to 110 ℃, heating at the rate of 0.5 ℃ per minute, and then preserving heat at 130 ℃ for 30 minutes;
(5) placing the dried composite material at 900 ℃ for sintering treatment for 1 hour;
(6) placing the sintered composite material in the mixed slurry for pressure impregnation, wherein the impregnation pressure is 4 MPa;
(7) and (3) placing the composite material after the slurry impregnation in a drying box for drying treatment. The drying treatment process comprises the steps of heating from room temperature to 110 ℃, heating at the rate of 0.5 ℃ per minute, and then preserving heat at 130 ℃ for 30 minutes;
(8) placing the dried composite material at 900 ℃ for sintering treatment for 1 hour;
(9) repeating the steps (3) to (8) for 5 times to obtain SiBN fiber reinforced SiO2-BN-Al2O3A fundamental wave-transparent composite material.
Example 3
(1) Preparing SiBN fiber into a 2.5-dimensional woven prefabricated part structure, wherein the fiber volume fraction of the prefabricated part is 45%;
(2) in SiO2Adding nanometer BN powder and nanometer Al into 30 mass percent of silica sol2O3Powder of, among them, silica sol, nano BN powder and nano Al2O3The mass ratio of the powder is 12:2:1, and after uniform stirring, mixed slurry is obtained, wherein SiO is contained in silica sol2The average particle diameter of the particles is 10-15 nm, the average particle diameter of the added nano BN is 100-200 nm, and nano Al2O3The average particle diameter of the particles is 30 to 60 nm.
(3) Placing the SiBN fiber prefabricated member in the mixed slurry for vacuum impregnation, wherein the impregnation pressure is 45 KPa;
(4) and (3) placing the SiBN fiber prefabricated member after the slurry impregnation into a drying box for drying treatment process. The drying treatment process comprises the steps of heating from room temperature to 115 ℃, heating at the rate of 1 ℃ per minute, and then preserving heat at 135 ℃ for 35 minutes;
(5) placing the dried composite material at 950 ℃ for sintering treatment for 2 hours;
(6) placing the sintered composite material in the mixed slurry for pressure impregnation, wherein the impregnation pressure is 6 MPa;
(7) and (3) placing the composite material after the slurry impregnation in a drying box for drying treatment. The drying treatment process comprises the steps of heating from room temperature to 115 ℃, heating at the rate of 1 ℃ per minute, and then preserving heat at 135 ℃ for 35 minutes;
(8) placing the dried composite material at 950 ℃ for sintering treatment for 2 hours;
(9) repeating the steps (3) to (8) for 6 times to obtain SiBN fiber reinforced SiO2-BN-Al2O3A fundamental wave-transparent composite material.
Example 4
(1) Preparing SiBN fiber into a 3-dimensional woven prefabricated part, wherein the fiber volume fraction of the prefabricated part is 50%;
(2) adding nanometer BN powder and nanometer Al into 30% silica sol2O3Powder is evenly stirred to obtain mixed slurry, and SiO in silica sol2The average particle diameter of the particles is 10-15 nm, the average particle diameter of the added nano BN is 100-200 nm, and nano Al2O3The average particle diameter of the particles is 30 to 60 nm. Wherein, the silica sol, the nanometer BN powder and the nanometer Al2O3Mass ratio of powder 12: 4: 1;
(3) placing the SiBN fiber prefabricated member in the mixed slurry for vacuum impregnation, wherein the impregnation pressure is 60 KPa;
(4) and (3) placing the SiBN fiber prefabricated member after the slurry impregnation into a drying box for drying treatment process. The drying treatment process comprises the steps of heating from room temperature to 120 ℃, heating at the rate of 1 ℃ per minute, and then preserving heat at 140 ℃ for 40 minutes;
(5) placing the dried composite material at 1000 ℃ for sintering treatment for 2 hours;
(6) placing the sintered composite material in the mixed slurry for pressure impregnation, wherein the impregnation pressure is 8 MPa;
(7) and (3) placing the composite material after the slurry impregnation in a drying box for drying treatment. The drying treatment process comprises the steps of heating from room temperature to 120 ℃, heating at the rate of 1 ℃ per minute, and then preserving heat at 140 ℃ for 40 minutes;
(8) placing the dried composite material at 1000 ℃ for sintering treatment for 2 hours;
(9) repeating the steps (3) to (8) for 4 times to obtain SiBN fiber reinforced SiO2-BN-Al2O3A fundamental wave-transparent composite material.
Claims (3)
1. SiBNFiber reinforced SiO2-BN-Al2O3The preparation method of the wave-transparent composite material comprises the following steps:
(1) adding nanometer BN and nanometer Al into silica sol2O3Uniformly stirring to obtain mixed slurry; wherein SiO in the silica sol2The mass percentage of (A) is 20-30%; SiO in silica sol2The average particle size of the particles is 10-15 nm; silica sol, nano BN and nano Al2O3The mass ratio of (8-12) to (1-4) to 1;
(2) placing the SiBN fiber prefabricated member in mixed slurry for vacuum impregnation, wherein the impregnation pressure is 20-60 KPa, and then drying and sintering to obtain a composite material after sintering; wherein the SiBN fiber prefabricated member is a 2.5-dimensional woven or 3-dimensional braided structure; the volume fraction of the fiber in the SiBN fiber prefabricated member is 35-50 percent;
(3) placing the sintered composite material in mixed slurry for pressure impregnation, wherein the impregnation pressure is 2-8 MPa, and then drying and sintering; wherein the sintering in the steps (2) and (3) is as follows: sintering at 800-1000 ℃ for 1-2 hours;
(4) repeating the steps (2) and (3) for 4-6 times to obtain SiBN fiber reinforced SiO2-BN-Al2O3A wave-transparent composite material.
2. SiBN fiber reinforced SiO according to claim 12-BN-Al2O3The preparation method of the wave-transparent composite material is characterized by comprising the following steps: the average grain diameter of the nanometer boron nitride BN in the step (1) is 100-200 nm, and the nanometer Al2O3The average particle diameter of the particles is 30 to 60 nm.
3. SiBN fiber reinforced SiO according to claim 12-BN-Al2O3The preparation method of the wave-transparent composite material is characterized by comprising the following steps: the drying in the steps (2) and (3) is as follows: raising the temperature from room temperature to 100-120 ℃, wherein the heating rate is 0.5-1 ℃ per minute, and then preserving the heat for 20-40 minutes at 120-140 ℃.
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| CN108149162A (en) * | 2017-12-27 | 2018-06-12 | 宁波市江北吉铭汽车配件有限公司 | A kind of high intensity guider |
| CN109696583B (en) * | 2019-02-26 | 2021-07-13 | 航天材料及工艺研究所 | Silicon nitride fiber sample for dielectric property test, sample preparation method and test method |
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